CN107352567A - Method for preparing high-purity aluminum oxide by vacuum reduction, distillation and purification - Google Patents
Method for preparing high-purity aluminum oxide by vacuum reduction, distillation and purification Download PDFInfo
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- CN107352567A CN107352567A CN201610299339.5A CN201610299339A CN107352567A CN 107352567 A CN107352567 A CN 107352567A CN 201610299339 A CN201610299339 A CN 201610299339A CN 107352567 A CN107352567 A CN 107352567A
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- fine powder
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- reducing agent
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000004821 distillation Methods 0.000 title claims abstract description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000000746 purification Methods 0.000 title abstract description 3
- 238000006722 reduction reaction Methods 0.000 title description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 55
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 14
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 14
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000003610 charcoal Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 241000894007 species Species 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The method for preparing high-purity aluminum oxide by vacuum reduction distillation purification can be used for purifying industrial grade Al with general purity2O3And (3) fine powder. The characteristic technology is as follows: the method comprises the following steps: (1) with Al of ordinary purity2O3Mixing it with high-purity fine powder of carbonaceous reducing agent in a certain proportion, (2) adding it into vacuum distillation furnace, vacuumizing to a certain vacuum degree, heating to a certain temp. and keeping it, and reduction distilling to make Al2O3Impurity of Na2O、SiO2、Fe2O3、TiO2、ZnO2MgO and CaO are reduced to metals by C in the fine powder of the carbonaceous reducing agent, and Na, Mg and Ca (and crystal H) are formed2O and CO2) Volatilize Al2O3Keeping the Fe solution unreduced, insoluble and volatile, and the Fe solution can be deposited on the A by gravityl2O3Then, (3) collecting the residue after reduction and evaporation, and removing the Fe liquid or solid Fe under the residue to obtain high purity Al2O3Fine powder, and collecting the condensed Na, Zn, Mg and Ca solutions of the evaporated gas by condensation respectively or in a mixed manner.
Description
Technical field
The present invention relates to the process that a kind of vacuum reduction distilation prepares high purity aluminium oxide.
Background technology
High-purity alchlor (Al2O3) it is important raw and processed materials required for the industries such as metallurgy, chemical industry, electronics, typically require its purity to be more than 4N levels;Sapphire crystal needed for LED industry has strict demand to the purity of aluminum oxide, particularly has particular/special requirement to micronutrient levels such as Si, Na, Ca, Mg, Cu, Ti, general to require it is that content is not more than 5ppm.According to《YS7274-1998》The Al of the industrial trade mark of production2O3Raw material (Al2O3- 1, -2, -3, -4, referred to as:Al2O3) purity be generally 2N levels, wherein containing impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO etc. (mainly first 4 kinds).It is existing to prepare high-purity Al2O3Method have:Zone melting method, the method equipment is complicated, needs in advance by Al2O3Bar, low production efficiency, cost height is made;Aluminium water direct hydrolysis method, the method technical process control are complicated, it is impossible to are purified, product purity depends on the purity of raw material aluminium fine powder;Alum method, advantage of lower cost, technique are simple, small investment, but produce discharge SO2Gas, pollutes environment, and product purity is low;Aluminium carbonate ammonium method, production cycle length, the bad control of technique, product purity is relatively low, in 4N or so;Aluminium alcoholates salt solution solution, the aluminum oxide purity of production is high, crystal grain is small, but cost height, complex technical process, safety and environmental issue be present;Vacuum cold crucible electromagnetic levitation-melt method, product purity in by raw material oxide impurity content influenceed.Currently without with common Al2O3Product is raw material, and high-purity Al is prepared by vacuum reduction distilation2O3Technology.According to non-ferrous metal vacuum reduction distillation principle, by vacuum reduction distillation certain reducing agent may be used to carry out reduction distillation purification to some metal oxides and prepare high purity metal oxides, product purity is expected to reach more than 4N or 5N levels, and process is simple, equipment is prior art, and cost is low.
Bibliography:
[1] Yongnian, Yang Bin nonferrous materials vacuum metallurgy [M] Beijing are worn:Metallurgical publishing house, 2000.
[2] Liu builds research [D] the Kunming University of Science and Technology thesis for the doctorate that people's pure aluminum Hydrolyze methods prepare high purity aluminium oxide, and 2005:1-40.
[3] Wang Jiao, Li Hongjun, bend skilful chivalrous, Xu Xiaodong, Zhang Daobiao, He Xuemei, and Xu Jun cold crucibles method prepares Al2O3Technological parameter research [J] artificial lens journals of polycrystalline material, 2012,41 (3):578-580.
[4] Lian Jiasong, Li Dongyun, Yang Hui.Green Synthesis of Nanometer γ-Al2O3 Powders by Sol-Gel Method [J] Rare Metals Materials and engineering.2008,37 (supplementary issues 2):334-336.
[5] preparation method [P] .CN201210403743.4 of a kind of α types nano-aluminium oxide particles of Luoyang Normal College,
The content of the invention
The object of the invention:
The present invention provides a kind of method that vacuum reduction distilation prepares high purity aluminium oxide, can be applied to prepare high purity aluminium oxide.
The technical solution of the present invention:
The method that vacuum reduction distilation prepares high purity aluminium oxide, it is characterized in that:It includes step:(1) using the Al of general purity2O3(abbreviation Al2O3), after it is well mixed according to a certain percentage with the carbonaceous reducing agent fine powder of high-purity, (2) are added in vacuum distillation furnace, and electrified regulation to certain temperature and is kept after vacuumizing up to certain vacuum degree, and carrying out reduction distillation makes described Al2O3In impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO (mainly first 4 kinds) be reduced to metal by the C in described carbonaceous reducing agent fine powder, and make Na, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding be not reduced and it is insoluble and volatilization, and Fe liquid can after stopping power supply gravity sedimentation in Al2O3Under, (3) collect the residue after described reduction and described evaporation, and remove the Fe liquid or solid-state Fe under described residue, obtain the high-purity Al of product2O3Powder, and condensing metal Na, Zn, Mg, Ca liquid of boil-off gas that can be respectively or described in condensation by mixing collection are byproduct.
The method that vacuum reduction distilation according to above-mentioned technical solution prepares high purity aluminium oxide, it is characterized in that:Described Al2O3Can be the Al of the industrial trade mark2O3Fine powder body;Described vacuum distillation furnace can carry the evaporator being made up of resistive heating device and crucible, and the single chamber or multiple-chamber type condenser being provided with according to the species of metal gas and its similarities and differences of dew point of volatilization;The carbonaceous reducing agent fine powder of described high-purity can be high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder;Described certain vacuum and temperature can be 10-1-10-2Pa and 1300-1200 DEG C;Described certain proportion can be according to described Al2O3Na described in fine powder2O、SiO2、Fe2O3、TiO2, ZnO, MgO, CaO accurately determine after accurately being calculated or tested by the required of the reduction completely of the C in described carbonaceous reducing agent fine powder.
The method that vacuum reduction distilation according to above-mentioned technical solution prepares high purity aluminium oxide, it is characterized in that:Described crucible can be corundum crucible.
Usefulness of the present invention:
Vacuum reduction distilation of the present invention prepares the technical method of high purity aluminium oxide, and according to aforementioned techniques solution, described Al can be made by step (1)-(4)2O3Impurity Na in fine powder2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO (mainly first 4 kinds) be reduced to metal by the carbonaceous reducing agent fine powder of high-purity, and make Na, Zn, Mg, Ca evaporative removal therein, but make Al2O3Holding is not reduced and insoluble and volatilization form residue, Fe liquid can gravity sedimentation, after the Fe liquid or solid-state Fe under the residue described in removing, obtain the Al of high-purity2O3Product, can also be in the single chamber or multiple-chamber type condenser described in different respectively or mixing recovery byproduct Na, Zn, Mg, Ca molten metal.Using the carbonaceous reducing agent fine powder of graphite fine powder or activated carbon fine powder or carbon black fines as described high-purity, it is ensured that it is high-purity and easily disperseed and described Al2O3Fine powder is well mixed according to described certain proportion, in favor of complete described reduction reaction occurs;Described certain vacuum and temperature and its be 10-1-10-2Pa and 1300-1200 DEG C, described Al can be both made2O3Described impurity Na in fine powder2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO be reduced, Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, Fe2O3Fe liquid is reduced to, described Al can be made again2O3Al in fine powder2O3Component is not reduced and occurs to volatilize and left behind, and after Fe liquid or solid-state Fe of the gravity sedimentation under described residue is removed, obtains high-purity Al2O3Fine powder product;Described certain proportion, it can both ensure that described reduction reaction occurred completely, by that can prevent in the high-purity Al of product2O3In have the impurity C compositions of residual;Described crucible is that corundum crucible can prevent it from being volatilized in described vacuum distillation or wherein impurity element pollutes the described high-purity Al of product2O3Fine powder;The single chamber or multiple-chamber type condenser being provided with according to the species of the metal gas of volatilization and its similarities and differences of dew point, it can make Na, Zn, Mg, Ca composition in described volatilization gas respectively or condensation by mixing is collected.The product purity prepared using the present invention is expected to reach more than 4N or 5N levels, and process is simple, and equipment is prior art, and cost is low.
Embodiment
Technical solution according to foregoing vacuum reduction distilation of the present invention prepares the technical method of high purity aluminium oxide:Can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace (prior art) described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion.Then:(1) using the Al of the industrial trade mark2O3Fine powder body (abbreviation Al2O3), after it is well mixed with the carbonaceous reducing agent fine powder high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder of described high-purity according to described certain proportion, (2) add in vacuum distillation furnace, it is 10 to vacuumize up to described certain vacuum-1-10-2Electrified regulation to described certain temperature is 1300-1200 DEG C and kept that carrying out reduction distillation makes described Al after Pa2O3In impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO metal is reduced to by the C in described carbonaceous reducing agent fine powder, and make Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding is not reduced and volatilizees and be in solid fine powder, and Fe be in a liquid state (can gravity sedimentation in Al2O3Under fine powder), (3) collect the residue after described reduction and described evaporation, after the Fe liquid or solid-state Fe under described residue is removed, you can obtain the high-purity Al of product2O3Fine powder, and can be in described single chamber or multiple-chamber type condenser, condensing metal Na, Zn, Mg, Ca liquid of the boil-off gas respectively or described in condensation by mixing collection are byproduct.
The application method of the present invention:
The above-mentioned technical solution and embodiment of the method for high purity aluminium oxide are prepared according to vacuum reduction distilation of the present invention, can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion;;Then, to the Al of the industrial trade mark2O3Described step (1) -- (3) are carried out, so as to prepare high-purity Al2O3Fine powder, and it is byproduct to collect metal Na, Zn, Mg, Ca liquid.
Embodiment one:The technical solution and embodiment of the invention described above of the technical method of high purity aluminium oxide are prepared according to vacuum reduction distilation of the present invention, can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion.Then:(1) using the Al of the industrial trade mark2O3Fine powder body (abbreviation Al2O3), after it is well mixed with the carbonaceous reducing agent fine powder high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder of described high-purity according to described certain proportion, (2) add in vacuum distillation furnace, it is 10 to vacuumize up to described certain vacuum-1Electrified regulation to described certain temperature is 1300 DEG C and kept that carrying out reduction distillation makes described Al after Pa2O3In impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO metal is reduced to by the C in described carbonaceous reducing agent fine powder, and make Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding is not reduced and volatilizees and be in solid fine powder, and Fe be in a liquid state (can gravity sedimentation in Al2O3Under fine powder), (3) collect the residue after described reduction and described evaporation, after the Fe liquid or solid-state Fe under described residue is removed, you can obtain the high-purity Al of product2O3Fine powder, and can be in described single chamber or multiple-chamber type condenser, condensing metal Na, Zn, Mg, Ca liquid of the boil-off gas respectively or described in condensation by mixing collection are byproduct.
Embodiment two:Vacuum reduction distilation according to the technical solution and embodiment of the invention described above prepares the technical method of high purity aluminium oxide, wherein one of described determine vacuum and described certain temperature for 10-2Pa and 1200 DEG C, remaining is identical with embodiment one.
Claims (3)
1. the method that vacuum reduction distilation prepares high purity aluminium oxide, it is characterized in that:It includes step:(1) using the Al of general purity2O3,
After it is well mixed according to a certain percentage with the carbonaceous reducing agent fine powder of high-purity, (2) are added in vacuum distillation furnace, are vacuumized up to certain vacuum degree
Electrified regulation to certain temperature and is kept afterwards, and carrying out reduction distillation makes described Al2O3In impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2、
MgO, CaO are reduced to metal by the C in described carbonaceous reducing agent fine powder, and make Na, Mg, Ca (and crystallization H2O) volatilize, but make
Al2O3Holding be not reduced and it is insoluble and volatilization, and Fe liquid can after stopping power supply gravity sedimentation in Al2O3Under, described in (3) collection also
Residue after former and described evaporation, and Fe liquid or solid-state Fe under described residue are removed, obtain the high-purity Al of product2O3Powder, and can divide
Condensing metal Na, Zn, Mg, Ca liquid of boil-off gas not or described in condensation by mixing collection are byproduct.
2. the method that vacuum reduction distilation according to claim 1 prepares high purity aluminium oxide, it is characterized in that:Described certain purity
Al2O3For the Al of the industrial trade mark2O3Fine powder body;Described vacuum distillation furnace carries the evaporator that is made up of resistive heating device and crucible, and according to
The species of the metal gas of volatilization and its similarities and differences of dew point and the single chamber or multiple-chamber type condenser being provided with;The carbonaceous reducing agent of described high-purity is thin
Powder is high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder;Described certain vacuum and temperature is 10-1-10-2Pa and
1300-1200℃;Described certain proportion is according to described Al2O3Na described in fine powder2O、SiO2、Fe2O3、TiO2、ZnO、MgO、
CaO is accurately determined after accurately calculating or test needed for the reduction completely of the C in described carbonaceous reducing agent fine powder.
3. the method that vacuum reduction distilation according to claim 2 prepares high purity aluminium oxide, it is characterized in that:Described crucible is corundum
Crucible.
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JPWO2020137875A1 (en) * | 2018-12-28 | 2021-11-25 | Dic株式会社 | Plate-shaped alumina particles, method for producing plate-shaped alumina particles, and resin composition. |
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CN104894382A (en) * | 2015-06-03 | 2015-09-09 | 东北大学 | Recovery treatment method of electrolytic aluminum ash and refractory material lining waste |
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JPWO2020137875A1 (en) * | 2018-12-28 | 2021-11-25 | Dic株式会社 | Plate-shaped alumina particles, method for producing plate-shaped alumina particles, and resin composition. |
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